反应详情

A solution of 5.4 g. of N-(p-fluorobenzyl)isatoic anhydride, 2.5 g. of 2-methylmercapto-imidazoline and one pellet (about 100 mg.) sodium hydroxide in 75 ml. of dioxane is refluxed with stirring for 4 hours. The resulting mixture is evaporated to dryness, the residue dissolved in methylene chloride, washed with water and extracted twice with 1N hydrochloric acid. The combined aqueous extracts are washed with methylene chloride and then with diethyl ether and made basic with sodium bicarbonate. The resulting precipitate is filtered off, washed thoroughly with water, dried by suction, dissolved in methylene chloride, dried with sodium sulfate, treated with charcoal and the methylene chloride exchanged for methanol to crystallize 10-(4'-fluorobenzyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one, m.p. 192°-195°C.

1. customThe resulting mixture is evaporated to dryness
2. dissolutionthe residue dissolved in methylene chloride
3. washwashed with water
4. extractionextracted twice with 1N hydrochloric acid
5. washThe combined aqueous extracts are washed with methylene chloride
6. filtrationThe resulting precipitate is filtered off
7. washwashed thoroughly with water
8. customdried by suction
9. dissolutiondissolved in methylene chloride
10. dry with materialdried with sodium sulfate
11. additiontreated with charcoal
12. customto crystallize 10-(4'-fluorobenzyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one, m.p. 192°-195°C.